Method of refining the soap floating on the waste-liquors obtained in the manufacture of sulphate- or sodium cellulose as well as sulphite waste-liquor



, cohol.

Patented Sept. 15, 1931 PATENT OFFICE CARL HENRIK MICHELSON, OF AIBO, FINLAND METHOD OF BEFIN'ING THE SOAP FLOATING ON THE WASTE-LIQUORS OBTAINED IN THE MANUFACTURE OF SULPHATE- WASTE-LIQ OR OB SODIUM CELLULOSE AS WELL AS SULPHITE Kc Drawing. Application filed April 19, 1929, Serial 110. 856,619, and in Finland Kay 9, 1928.

In the manufacture of sulphateor sodium cellulose, a saponaceous product is known to be formed, the same floating on the wasteliquor and consisting substantially of alkali salts of fatty or resinous acids. Out of this soap, as it is called, one has endeavoured to produce pure fatty and resinous acids in various ways. The product has been decomposed with acids, the fatty and resinous acids having thus been liberated, and forming a socalled floating rosin. This floating rosin has then been subjected to further purifying processes. The product has been distilled, and so forth, without it being possible, however, entirely to remove therefrom evil smelling and other contaminations.

According to the present invention, pure fatty and resinous acids are obtained from the soap, and at-the same time sulphite waste-liquor is refined. The method consists in that the soap, whether inthe crude state or urified in some way or other, is thoroug 1y stirred with sul room temperature or w ile being subjected to heating. The sulphite waste-liquor is used either as it is obtained in the manufacture of sulphite cellulose or in a more or less concentrated form, or, as a residue from the manufacture of sulphite yeast or sulphite al- The fatty and resinous acids contained in the soap and also in the sulphite waste-liquor are li erated and extracted from the mixture with the aid of a suitable solvent, such as benzine or the like. The solvent is expelled and a residue obtained in the form of a pure product consisting of fatty and resinacids then gradually formm ous acids which may be separated according to known methods. The extraction with the solvent may be efiected at room temperature or under heating. .It is also possible to proceed by leaving the mixture to sta after the soap has been thoroughly stirre with sulphite waste-liquor, the fatty and resinous the surface immed off or layer and permitting of being s in order separated in some other manner,

-then to be further purified-with a solvent or solvents, as above described. In' the process, the sulphite waste-liquor is also subjected to alteration. It brightens up considerably and hite waste-liquor at lutely dry residue.

0 The invention is illustrated by the following specific example, it being understood that the invention is not limited to the specific details described therein.

The sulphite waste-liquor used is withdrawn directly from a cellulose cooker and is cooled to 50 C. without addition of water. 750 to 1,000 liters of the waste-liquor are added to 100 kilograms of the so-called soap depending upon the degree of acidity of the waste-liquor. The soa and the waste liquor are mixed well for a out 1% hours in an open wooden vessel, the temperature being maintained at 50 C. during the entire time. Then the mixture is allowed to stand for about 1 hours. At the end of this time it will be found that the mixture has separated into two layers, the upper layer consisting of resinous and fatty substance, and the lower layer consisting of the changed sulphite waste liquor. The waste-liquor is drawn off through a drain in the bottom of the vessel and is then evaporated to dryness. The resinous and fatty substance remaining behind is subjected to a further purification process depending upon the use for which it is desired. For example, it is dissolved in benzine, the solution is filtered, and the, solvent is evaporated. Then, if desired, the resinous and fatty acids can be separated accordin to any of the methods known in the art. e fatty acid-resin acid mixture obtained in this process contains 93-95% of acids, of which 63 -5% are fatty acids, and 35-37% are resin ac1 s.

What I claim as new and desire to secure by Letters Patent of the United States of America is 1. In a process of recovering fatty and resinous acids from the so-ca1ledsoa floating on the waste-liquors obtained in t e manufactureof sulphateor sodium cellulose, the ste which comprises treating the said soap wit sulphite waste-liquor.

2. In a process of recovering oatv the step which comprises treating the said resinous acids from the so-called resinous acids from the so-called soap resinous acids from the so-called resinous acids from the so-called soa'p soap with sulphite waste-liquor at ordinary room temperature.

3. In a process of recovering fatty and soa floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose, the step which comprises treating the said soap with sulphite waste-liquor at a temperature above ordinary room temperature.

4. In a process of recovering fatty and resinous acids from the so-called soap floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose, the step whichcomprises treating the said soap with concentrated sulphite wasteliquor at ordinary room temperature.-

5. In a process of recoverin fatty and resinous acids from the so-ca led soap floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose, the step soap at ordinary room temperature with facture of sulphite cellulose.

resinous acids from the so-called soap oating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose, the step which comprises treating the said soap at a temperature above ordinary room temperature with sulphite waste-1i uor obtained in the manufacture of sulp 'te celulose. y

7. In a process of recoverin fatty and floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose,

the step which comprises treating the said soap with concentrated sulphite waste-liquor at a'temperature above ordinary room temperature. a

8. In a process of recovering fatt and ing on thewaste-liquors obtainadin the manufacture of sulphateor sodium cellulose,

the step which comprises treating the said soa at ordinary room temperature with sulp ite waste-liquor obtained in the manufacture of sulphite yeast. 7 9. In a process of recovering fatty and resinous acids from the so-called soap floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose, the step which comprises treating the said soa at ordinary room temperature with sulp ite'waste-liquor obtained in the manu-- facture of sulphite alcohol.

- 10, In a process of recovering fatty and floating on the waste-liquors obtained in the manufacture of sulphateor sodium cellulose the step which comprises treating the said manufacture of sulphatewhich comprises treating the said.

solvent and sulphite waste-liquor obtained in the manu- I soap at a temperature above ordinary room temperature with sulphite waste-liquor obtained in the manufacture of sulphite yeast.

11. In a rocess of recovering fatty and resinous aci s from the so-called soap floating on the waste-liquors obtained in the or sodium cellulose, the step which comprises treating the said soap at a temperature above ordinary room temperature with sulphite waste-liquor obtained in the manufacture of sulphite alcohol.

12. A rocess as claimed in claim 1 wherein the li rated fatty and resinous acids are extracted with an organic solvent and the solvent is then evaporated.

1 3. In a process of recovering fatty and resinous aci s from the so-called soap floating on the. 'waste-liquors obtained in, the

, manufacture of sulphateor sodium cellulose,

the steps :which com rise, treating'the said soap with, sulphite waste-liquor, allowing the mixture tostand until it separates into two la ers, extracting the resinous and fatty acids rom the upper layer with an organic evaporating the said solvent. In testimony whereof I afiix my signature.

CARL HENRIK MICHELSON'. 

